The present invention relates to an improved liquid-liquid solvent extraction process for removing and recovering Zn or Cd and cyanide values from cyanide solutions, such as those produced from electroplating aqueous effluents. These include, but are not limited to, spent electroplating solutions as well as relatively larger volumes of rinse waters used to rinse electroplated parts to remove cyanide therefrom. In previous years such effluents were routinely discharged to public water. Today, environmental standards imposed by federal, state, and municipal laws and regulations impose increasing rigorous requirements on the maximum permissible cyanide and toxic levels of Zn or Cd contained in aqueous effluents discharged into public streams.